CN106749376A - The linear polysiloxane composition and preparation method of different rate of volatilizations - Google Patents

The linear polysiloxane composition and preparation method of different rate of volatilizations Download PDF

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Publication number
CN106749376A
CN106749376A CN201611237557.2A CN201611237557A CN106749376A CN 106749376 A CN106749376 A CN 106749376A CN 201611237557 A CN201611237557 A CN 201611237557A CN 106749376 A CN106749376 A CN 106749376A
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linear polysiloxane
composition
volatilizations
purity
different rate
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孙宇
尹迎阳
马宏明
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JIANGSU MAYSTA CHEMICAL CO Ltd
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JIANGSU MAYSTA CHEMICAL CO Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/58Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
    • A61K8/585Organosilicon compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02Silicon compounds
    • C07F7/08Compounds having one or more C—Si linkages
    • C07F7/0834Compounds having one or more O-Si linkage
    • C07F7/0838Compounds with one or more Si-O-Si sequences
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02Silicon compounds
    • C07F7/08Compounds having one or more C—Si linkages
    • C07F7/0834Compounds having one or more O-Si linkage
    • C07F7/0838Compounds with one or more Si-O-Si sequences
    • C07F7/0872Preparation and treatment thereof
    • C07F7/0874Reactions involving a bond of the Si-O-Si linkage
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02Silicon compounds
    • C07F7/08Compounds having one or more C—Si linkages
    • C07F7/20Purification, separation
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10General cosmetic use

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention belongs to chemical process technical field, more particularly to the linear polysiloxane composition with different rate of volatilizations, the present invention is with organosilicon mixture as raw material, obtained with volatile high-purity linear polysiloxane by complicated separating technology, the organosilicon mixture by organosilicon ring and HMDO in acid condition balanced reaction and obtain.The present invention is with two kinds or the combination of two or more high-purity linear polysiloxanes obtains the linear polysiloxane composition of different rate of volatilizations, and the composition rate of volatilization has controllability, widens its application field.

Description

The linear polysiloxane composition and preparation method of different rate of volatilizations
Technical field
The invention belongs to chemical process technical field, more particularly to a kind of linear polysiloxane with different rate of volatilizations And preparation method thereof.
Background technology
Dimethyl silicone polymer is used frequently as cosmetics because of the boiling characteristics of its good disperse properties and uniqueness Volatile ingredient.It is limpid, tasteless, substantially odorless, without greasy feeling.With other volatility used in personal care industries Unlike carrier, this volatile organosilicon oil will not be made due to the relatively low reason of its volatilization temperature in evaporation Skin cools off.
Cyclic polysiloxanes are the volatile ingredients of usually used cosmetics, including such as octamethylcy-clotetrasiloxane (D4), the analog such as decamethylcyclopentasiloxane (D5) and the siloxanes of ten diformazan basic ring six (D6).Although however, D4 show it is excellent Good volatility, but because the freezing point of D4 only has 17~18 DEG C, easily crystallization, causes cryopreservation to include D4 at low ambient temperatures Cosmetics in the case of, influence is used.And D5 has no problem in terms of cryopreservation stability, but its volatility is not strong, and Due to the reason so that the sense of touch during the cosmetics use comprising D5 is thick and heavy, shows viscosity, it is impossible to which acquisition uses process In good feel problem.Corresponding, the volatility of D6 is weaker, and the thick and heavy sense during use is stronger.
In view of above mentioned problem, WO01/15658 proposes a kind of structure for [(CH3)3SiO]3SiCH3The poly- trimethyl of methyl Siloxanes, it can be as volatile ingredient in cosmetics.Although however, being blended organic poly- described in WO01/15658 The cosmetics of siloxanes show good volatility, but it fails to sufficiently improve the sense of touch during use, and especially, not Can fully avoid drying the problem of sensation.Accordingly, it would be desirable to the further improvement on above mentioned problem.
A kind of new organopolysiloxane with ad hoc structure is provided in CN102639542A and comprising above-mentioned organic The cosmetics of polysiloxanes.Point out that this new organopolysiloxane is volatile in patent, with low-temperature stability, there is provided Excellent glossiness, and with the premium properties with the miscibility of ultra-violet absorber, and the organopolysiloxane conduct The sub of octamethylcy-clotetrasiloxane, decamethylcyclopentasiloxane or the poly- trimethicone of methyl is useful.But synthesis Complex process, process is difficult to control, and is not suitable for industrialized production.
The linear polysiloxane of corresponding low polymerization degree has less viscosity, excellent volatility and low-temperature storage stabilization Property etc..The preparation method to the linear poly- silica of the high-purity with different rate of volatilizations and combinations thereof not yet has related report at present Road.
The content of the invention
It is an object of the invention to provide the linear polysiloxane composition with different rate of volatilizations.It is of the invention another Purpose is to provide the preparation method of the linear polysiloxane with different rate of volatilizations.
Linear polysiloxane composition with different rate of volatilizations of the present invention, further technical scheme is institute It is a kind of linear polydimethylsiloxane- to state linear polysiloxane, with following (I) formula structural formula:
(I) the corresponding structure of formula is abbreviated as MDmM, wherein, m is 1~6 integer.
The composition is made up of two or more linear polysiloxane, and linear polysiloxane is described in composition The linear polysiloxane of high-purity.
Linear polysiloxane composition with different rate of volatilizations of the invention, its further technical scheme can be with It is that the composition is stirred at normal temperatures and pressures with arbitrary proportion by the linear polysiloxane of two or more high-purity It is obtained by mixing.
Linear polysiloxane composition with different rate of volatilizations of the invention, its further technical scheme can be with It is that the linear polysiloxane of the high-purity refers to the material that purity is 99%~100% after testing.
Linear polysiloxane composition with different rate of volatilizations of the invention, its further technical scheme can be with It is that the rate of volatilization is measured according to DIN chemistry meeting DIN53170-2009 standards.
The linear polysiloxane of high-purity of the present invention has volatility.
Present invention also offers a kind of linear polysiloxane preparation method of the high-purity:Comprise the following steps, raw material By normal pressure, decompression separation technique, the linear polysiloxane with different rate of volatilizations with high-purity is obtained;
The preparation method of the linear polysiloxane with different rate of volatilizations of the invention, its further technical scheme is also Can be that described raw material is organosilicon mixture, come from organosilicon ring with HMDO in acid condition Balanced reaction and obtain, further described organosilicon ring is hexamethyl cyclotrisiloxane (D3), the silica of prestox ring four Alkane (D4), decamethylcyclopentaandoxane (D5), one or more mixture of the siloxanes of ten diformazan basic ring six (D6).
Linear polysiloxane composition with different rate of volatilizations of the invention, its further technical scheme can be with The rate of volatilization for being described composition is adjustable, preferably by the ratio of each component in regulation composition.
According to another aspect of the present invention, the invention provides a kind of linear polysiloxane combination of different rate of volatilizations The preparation method of thing, comprises the following steps:
1) the corresponding height of (1) formula in claim 1 is prepared by normal pressure, decompression separation by raw material of organosilicon mixture The linear polysiloxane of purity;
2) two or more step 1) the linear polysiloxane of high-purity stirred at normal temperatures and pressures with arbitrary proportion Mix mixing
The present invention has advantage following prominent and good effect:
The linear polysiloxane composition that the present invention is provided has different rate of volatilizations, can be used as a kind of volatility silicon Oil, and its rate of volatilization has controllability, widens its application field.
Brief description of the drawings
Fig. 1 is the rate of volatilization of the linear polysiloxane of different structure prepared by the present invention;
Fig. 2 is the rate of volatilization of the linear polysiloxane composition of different structure prepared by the present invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, with reference to specific embodiment, to this Invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the present invention.
Embodiment 1
Organosilicon mixture enter rectifying column in, under the conditions of certain vacuum, raw material be heated vaporization after, steam Ta Nei with The liquid of overhead condenser backflow carries out gas-liquid mass transfer on filler surface, carries out rectifying separation;Rectifying column tower top obtains gas phase, warp Condenser is condensed, and by adjusting reflux ratio, the qualified material of extraction purity obtains the line of different structure through pipeline to storage tank Property polysiloxanes.
(1) MDM for obtaining, is 99.86% through gas chromatographic detection purity.
(2) MD for obtaining2M, is 99.88% through gas chromatographic detection purity.
(3) MD for obtaining3M, is 99.92% through gas chromatographic detection purity.
(4) MD for obtaining4M, is 99.78% through gas chromatographic detection purity.
(5) MD for obtaining5M, is 99.57% through gas chromatographic detection purity.
(6) MD for obtaining6M, is 99.81% through gas chromatographic detection purity.
Embodiment 2
The linear of high-purity obtained in case study on implementation 1 is gathered according to DIN chemistry meeting DIN53170-2009 standards Siloxanes (m=1~6) measures rate of volatilization, as a result as shown in Figure 1:
The linear polysiloxane MDM, MD of the high-purity to obtaining2M, MD3M, MD4M, MD5M, MD6M carries out rate of volatilization survey Amount, as a result finds, the rate of volatilization of the linear polysiloxane of different structure is MDM>MD2M>MD3M>MD4M>MD5M>MD6M, with The chain link of linear polysiloxane gradually increases, and its rate of volatilization slows down gradually.
Case study on implementation 3
The volatilization of composition prepared by the linear polysiloxane (m=1~6) according to the high-purity obtained in case study on implementation 1 Speed is as shown in Figure 2:Wherein
Composition 1:According to weight ratio, MDM50%, MD2M50%.
Composition 2:According to weight ratio, MDM60%, MD3M40%.
Composition 3:According to weight ratio, MDM60%, MD2M38%, MD3M2%.
Composition 4:According to weight ratio, MDM52%, MD2M35%, MD3M13%.
Composition 5:According to weight ratio, MDM40%, MD3M40%, MD4M15%, MD5M5%.
Composition 6:According to weight ratio, MDM24%, MD3M38%, MD5M6%, MD6M32%.
Composition 7:According to weight ratio, MDM14%, MD3M46%, MD5M5%, MD6M35%.
Rate of volatilization measurement is carried out to 7 kinds of linear polysiloxane compositions of various combination, is as a result found, composition Rate of volatilization can be to be adjusted according to the ratio of each component in composition.Wherein, the chain link of linear polysiloxane is shorter, its Rate of volatilization is faster, its in the composition proportion it is bigger, rate of volatilization is faster;Conversely, its proportion in the composition Fewer, rate of volatilization is slower.The chain link of linear polysiloxane is more long, and its rate of volatilization is slower, its proportion in the composition Smaller, rate of volatilization is faster;Conversely, its in the composition proportion it is bigger, rate of volatilization is slower.
Although embodiments of the present invention are described in detail, it should be understood that, without departing from of the invention In the case of spirit and scope, embodiments of the present invention can be made with various changes, replace and change.

Claims (8)

1. a kind of linear polysiloxane composition with different rate of volatilizations, the linear polysiloxane is that structural formula is (I) Shown linear polydimethylsiloxane-:
The wherein corresponding structure of (I) formula is abbreviated as MDmM, wherein, m is 1~6 integer;
The composition is made up of two or more linear polysiloxane, and linear polysiloxane described in composition is high-purity The linear polysiloxane of degree.
2. the linear polysiloxane composition with different rate of volatilizations according to claim 1, it is characterised in that:It is described Composition be by the linear polysiloxane of two or more high-purity with arbitrary proportion at normal temperatures and pressures stir mixing and .
3. the linear polysiloxane composition with different rate of volatilizations according to claim 1, it is characterised in that:It is described The linear polysiloxane of high-purity refers to the material that purity is 99%~100% after testing.
4. the linear polysiloxane composition with different rate of volatilizations according to claim 1, it is characterised in that:It is described Rate of volatilization is measured according to DIN chemistry meeting DIN53170-2009 standards.
5. the linear polysiloxane composition with different rate of volatilizations according to claim 1, it is characterised in that:It is described The linear polysiloxane of high-purity has volatility.
6. the linear polysiloxane composition with different rate of volatilizations according to claim 1, it is characterised in that:It is described The linear polysiloxane of high-purity is prepared by following preparation methods:Comprise the following steps, raw material is by normal pressure, decompression separation work Skill, obtains the linear polysiloxane with different rate of volatilizations with high-purity;
Described raw material is organosilicon mixture, and the organosilicon mixture is existed by organosilicon ring and HMDO Balanced reaction under acid condition and obtain;Described organosilicon ring be hexamethyl cyclotrisiloxane, octamethylcy-clotetrasiloxane, One or more of decamethylcyclopentaandoxane, the siloxanes of ten diformazan basic ring six.
7. the linear polysiloxane composition with different rate of volatilizations according to claim any one of 1-6, its feature It is:The rate of volatilization of the composition is adjustable, and rate of volatilization is by linear polysiloxane component in regulation composition Realized with ratio.
8. the preparation method of the linear polysiloxane composition with different rate of volatilizations described in a kind of claim 1, including Following steps:
1) the corresponding high-purity of (1) formula in claim 1 is prepared by normal pressure, decompression separation by raw material of organosilicon mixture Linear polysiloxane;
2) two or more step 1) the linear polysiloxane of high-purity stir mixed at normal temperatures and pressures with arbitrary proportion Close.
CN201611237557.2A 2016-12-28 2016-12-28 The linear polysiloxane composition and preparation method of different rate of volatilizations Pending CN106749376A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113522361A (en) * 2020-04-22 2021-10-22 江西蓝星星火有机硅有限公司 Immobilized catalyst for purifying cyclosiloxane

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5059578A (en) * 1973-10-02 1975-05-22
CN1051671A (en) * 1989-10-11 1991-05-29 理查森-维克斯有限公司 Improved facial cleansing compositions
CN1169109A (en) * 1994-12-15 1997-12-31 埃斯蒂劳德公司 Stable water-in-oil emulsion system
CN1247868A (en) * 1998-08-20 2000-03-22 瓦克化学有限公司 Volatile linear siloxanes mixture

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5059578A (en) * 1973-10-02 1975-05-22
CN1051671A (en) * 1989-10-11 1991-05-29 理查森-维克斯有限公司 Improved facial cleansing compositions
CN1169109A (en) * 1994-12-15 1997-12-31 埃斯蒂劳德公司 Stable water-in-oil emulsion system
CN1247868A (en) * 1998-08-20 2000-03-22 瓦克化学有限公司 Volatile linear siloxanes mixture

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JULIAN CHOJNOWSKI ET AL.: "Cationic Polymerization of Siloxanes Kinetically Controlled Oligomerization in Hexamethyl-cyclotrisiloxane-Linear Dimethylsiloxane Systems", 《MAKROMOL. CHEM.》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113522361A (en) * 2020-04-22 2021-10-22 江西蓝星星火有机硅有限公司 Immobilized catalyst for purifying cyclosiloxane

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Application publication date: 20170531